Water → HCID 22170232、化合物
反応式
[NH2:1][C:2]1[C:3]([CH2:12][CH3:13])=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5](OC)=[O:6].[H-].[Al+3].[Li+].[H-].[H-].[H-].O>C1COCC1>[NH2:1][C:2]1[C:3]([CH2:12][CH3:13])=[C:4]([CH2:5][OH:6])[CH:9]=[CH:10][CH:11]=1参加物
5
実験手順
To a solution of methyl 3-amino-2-ethylbenzoate (0.83 g, 4.63 mmol), in THF (40 ml) was added Lithium aluminium hydride (0.9 g, 23.7 mmol). The mixture was heated at 50 C. for 5 h, cooled to 0 C. and hydrolysed cautiously with water. The slurry was extracted with EtOAc (×5). The extracts were washed with brine, dried Na2SO4, and evaporated. The residue was purified by chromatography (CH2Cl2/MeOH) to give the title compound 0.63 g (89%) as a white powder.
後処理
- temperatureThe mixture was heated at 50 C
- temperaturecooled to 0 C
- extractionThe slurry was extracted with EtOAc (×5)
- washThe extracts were washed with brine, dried Na2SO4
- customevaporated
- customThe residue was purified by chromatography (CH2Cl2/MeOH)
出典と根拠
- ORDレコード
- ord-a9d2c71466414e4ea5eb150388f3719c
- 出典データセット
- uspto-grants-2006_05
- 特許番号
- US07037925B2
反応ノート
読み込み中…